CN115637078A - Preparation method of intumescent carbon layer thickness-controllable flame retardant and flame-retardant wood - Google Patents
Preparation method of intumescent carbon layer thickness-controllable flame retardant and flame-retardant wood Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 97
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000002023 wood Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 235000002949 phytic acid Nutrition 0.000 claims abstract description 64
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims abstract description 63
- 239000007787 solid Substances 0.000 claims abstract description 36
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000004202 carbamide Substances 0.000 claims abstract description 35
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229940068041 phytic acid Drugs 0.000 claims abstract description 33
- 239000000467 phytic acid Substances 0.000 claims abstract description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 30
- 229920002472 Starch Polymers 0.000 claims abstract description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008107 starch Substances 0.000 claims abstract description 25
- 235000019698 starch Nutrition 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 22
- 239000000543 intermediate Substances 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229960000583 acetic acid Drugs 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000008014 freezing Effects 0.000 claims abstract description 7
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims description 13
- 229920001592 potato starch Polymers 0.000 claims description 7
- 229920002261 Corn starch Polymers 0.000 claims description 3
- 240000003183 Manihot esculenta Species 0.000 claims description 3
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229940100445 wheat starch Drugs 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 13
- 238000000576 coating method Methods 0.000 abstract description 13
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 21
- 239000000779 smoke Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 10
- 241000219000 Populus Species 0.000 description 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- -1 ammonium phytates Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
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- 230000003247 decreasing effect Effects 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of wood processing, and particularly relates to a flame retardant with controllable thickness of an expanded carbon layer and a preparation method of flame-retardant wood, wherein the preparation method of the flame retardant comprises the following steps: putting phytic acid and urea into a reaction container, heating, condensing and refluxing to obtain oily liquid; freezing the oily liquid in ultralow temperature equipment; drying by using a freeze dryer to obtain a solid intermediate; adding the solid intermediate, starch and glacial acetic acid into pure water, and heating and stirring to obtain the required flame retardant; coating the flame retardant on the raw material wood, drying in the shade, drying and balancing water to obtain the flame-retardant wood. The method adopts phytic acid and urea as raw materials to obtain ammonium phytate with different reaction degrees; the aim of regulating and controlling the thickness of the starch-based flame-retardant expanded carbon layer is achieved by utilizing different proportions of phytic acid, ammonium phytate and urea, and the application of the starch-based expanded flame retardant in serving as a wood flame retardant is expanded.
Description
Technical Field
The invention belongs to the technical field of wood processing, and particularly relates to a flame retardant with a controllable thickness of an expanded carbon layer and a preparation method of flame-retardant wood.
Background
The wood is used as a natural degradable environment-friendly material and plays an important role in the life of people. But its use is greatly limited due to its flammability. Therefore, the wood is modified while the excellent performance of the wood is exerted, the flame retardant property of the wood is improved, the application range of the wood is expanded, and the wood-modified wood is an important way for saving wood resources and meeting various functional requirements of people in life.
With the recent increase in the demand for flame retardancy and the growing awareness of environmental protection, the non-halogenation, smoke suppression and attenuation of flame retardants have become leading issues in the field of flame retardant research currently and in the future. Compared with the traditional flame retardant, the flame retardant has the serious defects of large addition amount, large smoke generation amount, toxic and corrosive gas generation and the like and is being replaced by a new generation of environment-friendly flame retardant. The intumescent flame retardant is a novel composite flame retardant which is widely concerned in the field of flame retardance in China in recent years. It has unique fire retardant mechanism and no halogen, low smoke and low toxicity, and is one important non-halogenated way of fire retardant. The expansion flame-retardant system forms a compact porous foam carbon layer on the surface of the material during combustion due to the synergistic effect of the acid source, the carbon source and the gas source. Not only can prevent the inner layer high polymer from further degrading and the combustible from releasing to the surface, but also can prevent the heat source from transmitting to the high polymer and isolate the oxygen source, thereby preventing the spread and propagation of flame. The intumescent flame retardant has the advantages of excellent flame retardant property, no halogen, low smoke, low toxicity, molten drop prevention and no corrosive gas, conforms to the development direction of the future flame retardant, and has very wide development prospect.
However, the existing intumescent flame retardant still has the defects when being used as a wood flame retardant, and the thickness of the intumescent carbon layer of the intumescent carbon flame retardant can not be effectively controlled, so that the application of the intumescent carbon flame retardant is limited. Therefore, it is necessary to provide a flame retardant with controllable thickness of an expanded carbon layer and a method for preparing flame-retardant wood using the same.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a flame retardant with a controllable thickness of an expanded carbon layer and a preparation method of flame-retardant wood.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
the invention provides a flame retardant with controllable thickness of an expanded carbon layer, and a preparation process of the flame retardant comprises the following steps:
1) Putting phytic acid and urea into a reaction vessel according to a certain molar ratio, heating, condensing and refluxing for 4-8 h at the temperature of 90-130 ℃ to obtain oily liquid;
2) Putting the obtained oily liquid into ultralow temperature equipment, and freezing at the temperature of minus 80 ℃ for 12-48 h; then drying for 12-48 h at-50 ℃ by using a freeze dryer to obtain a solid intermediate;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into a proper amount of pure water according to a certain mass ratio, and heating and stirring at the temperature of 85-95 ℃ for 5-20 min to obtain the required flame retardant.
Further, the molar ratio of the phytic acid to the urea is 1 x, wherein x = 3-20;
when x =6, the solid intermediate obtained in step 2) is an ammonium phytate solid;
when x is less than 6, the solid intermediate obtained in the step 2) is phytic acid/ammonium phytate composite solid;
when x is larger than 6, the solid intermediate obtained in the step 2) is urea/ammonium phytate composite solid.
Further, in step 1), heating and condensing reflux are carried out for 6h at the temperature of 120 ℃.
Further, in step 2), the obtained oily liquid is put into an ultralow temperature device and is frozen at the temperature of minus 80 ℃ for 24 hours.
Further, in step 2), drying at-50 ℃ for 24h by using a freeze dryer.
Further, in the step 3), the mixture is heated and stirred for 5-20 min at the temperature of 85-95 ℃.
Further, in the step 3), the starch is at least one of potato starch, corn starch, tapioca starch and wheat starch.
Further, in the step 3), the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 5-15.
Further, the mass ratio of the solid intermediate, starch and glacial acetic acid is 10.
The invention also provides a method for preparing flame-retardant wood by using the expandable carbon layer thickness-controllable flame retardant, which comprises the following steps:
s1, firstly, the flame retardant is mixed according to the proportion of 0.20-0.30 g/cm 2 Smearing on the raw material wood board;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and then drying at 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood plate in a constant temperature and humidity box, and carrying out water balance at the temperature of 22 ℃ and the humidity of 65%, wherein the balance time is more than or equal to 80h.
The invention has the beneficial effects that:
the method adopts phytic acid and urea as raw materials to obtain ammonium phytate with different reaction degrees, wherein the phytic acid is used as an acid source, the ammonium phytate is used as the acid source and an air source, and the urea is used as the air source; the aim of regulating and controlling the thickness of the starch-based flame-retardant expanded carbon layer is achieved by utilizing different proportions of phytic acid, ammonium phytate and urea, and the application of the starch-based expanded flame retardant as a wood flame retardant is expanded.
Of course, it is not necessary for any product to achieve all of the above advantages at the same time in the practice of the invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is an infrared plot of the groups of ammonium phytates of examples 1-7;
FIG. 2 is a graph of smoke density rating for comparative examples 1-2, examples 1-7;
FIG. 3 is a schematic diagram of the reaction between phytic acid and urea.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a flame retardant with controllable thickness of an expanded carbon layer, and a preparation process of the flame retardant comprises the following steps:
1) Putting phytic acid and urea into a reaction vessel according to a certain molar ratio, heating at 90-130 ℃, condensing and refluxing for 4-8 h to obtain oily liquid;
2) Putting the obtained oily liquid into ultralow temperature equipment, and freezing at the temperature of minus 80 ℃ for 12-48 h; then drying for 12-48 h at-50 ℃ by using a freeze dryer to obtain a solid intermediate;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into a proper amount of pure water according to a certain mass ratio, and heating and stirring at the temperature of 85-95 ℃ for 5-20 min to obtain the required flame retardant.
In the invention, the molar ratio of the phytic acid to the urea is 1 x, wherein x = 3-20;
when x =6, the solid intermediate obtained in step 2) is an ammonium phytate solid;
when x is less than 6, the solid intermediate obtained in the step 2) is phytic acid/ammonium phytate composite solid;
when x is larger than 6, the solid intermediate obtained in the step 2) is urea/ammonium phytate composite solid.
In the invention, the starch is at least one of potato starch, corn starch, cassava starch and wheat starch.
In the invention, the mass ratio of the solid intermediate, the starch and the glacial acetic acid is 5-15.
The method for preparing the flame-retardant wood by using the expandable carbon layer thickness-controllable flame retardant comprises the following steps:
s1, firstly, the flame retardant is mixed according to the proportion of 0.20-0.30 g/cm 2 (wherein the coating amount of the effective components of the flame retardant is 0.035-0.052 g/cm 2 ) Smearing on raw wood boards;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and then drying at the temperature of 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood board in a constant temperature and humidity box, and carrying out water balance under the conditions of temperature of 22 ℃ and humidity of 65%, wherein the balance time is more than or equal to 80h.
The method adopts phytic acid and urea as raw materials to obtain the ammonium phytate with different reaction degrees, and the reaction mechanism is shown in figure 3, wherein the phytic acid is used as an acid source, the ammonium phytate is used as the acid source and an air source, and the urea is used as the air source.
The specific embodiment of the invention is as follows:
example 1
1) Preparation of phytic acid/ammonium phytate composite flame retardant
Putting phytic acid and urea into a three-neck flask according to a molar ratio of 1. Then putting into an ultra-low temperature refrigerator with the temperature of 80 ℃ below zero for freezing for 24 hours. And then drying for 24 hours at minus 50 ℃ by using a freeze dryer to obtain the phytic acid/ammonium phytate composite flame retardant in a white solid state, wherein the molar ratio of the phytic acid to the ammonium phytate is 1.
2) Preparation of flame-retardant coating
Dissolving 10g of potato starch, 10g of phytic acid/ammonium phytate composite flame retardant solid and 1g of glacial acetic acid in 100g of pure water, and heating and stirring at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained in the above way is mixed according to the proportion of 0.25g/cm 2 The adhesive is smeared on a poplar sample, and the sample specification is 100mm in length, 50mm in width and 5mm in thickness. The smeared sample is placed in a fume hood to be dried in the shade for 3h, then placed in a blast drying oven to be dried at 40 ℃, and then placed in a constant temperature and humidity box with the temperature of 22 ℃ and the humidity of 65 percent to be balanced for 88h.
Example 2
1) Preparation of ammonium phytate flame retardant
Putting phytic acid and urea into a three-neck flask according to a molar ratio of 1. Then putting into an ultra-low temperature refrigerator of minus 80 ℃ for freezing for 24h. Then drying for 24h at minus 50 ℃ by using a freeze dryer to obtain the white ammonium phytate.
2) Preparation of flame-retardant coating
10g of potato starch, 10g of ammonium phytate flame retardant solid and 1g of glacial acetic acid are dissolved in 100g of pure water, and the mixture is heated and stirred at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained above is mixed according to the proportion of 0.25g/cm 2 (wherein the effective coating amount of the flame retardant is 0.043g/cm 2 ) The adhesive is smeared on a poplar sample, and the sample specification is 100mm in length, 50mm in width and 5mm in thickness. The smeared sample is placed in a fume hood to be dried in the shade for 3h, then placed in a blast drying oven to be dried at 40 ℃, and then placed in a constant temperature and humidity box with the temperature of 22 ℃ and the humidity of 65 percent to be balanced for 88h.
Example 3
1) Preparation of urea/ammonium phytate composite flame retardant
Putting phytic acid and urea into a three-neck flask according to a molar ratio of 1. Then putting into an ultra-low temperature refrigerator of minus 80 ℃ for freezing for 24h. And then drying for 24 hours at the temperature of minus 50 ℃ by using a freeze dryer to obtain the white solid urea/ammonium phytate composite flame retardant.
2) Preparation of flame-retardant coating
Dissolving 10g of potato starch, 10g of urea/ammonium phytate composite flame retardant solid and 1g of glacial acetic acid in 100g of pure water, and heating and stirring at 90 ℃ for 10min to obtain the flame retardant coating.
3) Flame retardant wood preparation
The intumescent flame retardant obtained above is mixed according to the proportion of 0.25g/cm 2 (wherein the effective coating amount of the flame retardant is 0.043g/cm 2 ) The adhesive is smeared on a poplar sample, and the specification of the sample is 100mm in length, 50mm in width and 5mm in thickness. The smeared sample is placed in a fume hood for drying in the shade for 3h, then placed in a blast drying oven for drying at 40 ℃, and then placed in a constant temperature and humidity box with the temperature of 22 ℃ and the humidity of 65% for balancing for 88h.
Example 4
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1.
Example 5
The present example is substantially the same as example 3, except that the molar ratio of phytic acid to urea is 1.
Example 6
This example is essentially the same as example 3, except that the molar ratio of phytic acid to urea is 1.
Example 7
This example is substantially the same as example 3 except that the molar ratio of phytic acid to urea is 1.
Comparative example 1
The poplar material is untreated, and the specification of the poplar material is 100mm in length, 50mm in width and 5mm in thickness.
Comparative example 2
Dissolving 10g potato starch and 1g acetic acid in 100g pure water, stirring and heating at 90 deg.C for 10min to obtain starch coating, wherein the weight ratio of the starch coating to the pure water is 0.25g/cm 2 The adhesive is uniformly coated on the surface of a poplar sample, and the sample specification is 100mm long, 50mm wide and 5mm thick.
Fourier infrared testing
The chemical structure of the ammonium phytate starch coating was characterized using a fourier transform infrared spectrometer. The sample preparation method is KBr tablet pressing method, and the wave number scanning range is 400-4000cm -1 The number of scanning times is 32, and the resolution is 4cm -1 。
The infrared curve of each ammonium phytate group is shown in FIG. 1, and it can be seen that at 1450cm -1 And 3210cm -1 The stronger absorption peak is formed by NH 4+ Is caused by bending and stretching vibration of (2) and is simultaneously 1050cm -1 、965cm -1 Characteristic peaks of P-O and P = O appear at the positions, and the experimental phenomenon can prove that PA and Urea successfully react to generate the ammonium phytate.
The symbols in the drawings mean: 1-3 represents that the molar ratio of phytic acid to urea as the reaction raw materials is 1, 3,1-6, 1-9, 1-12, 1-15, 1-18 and 1-20, and is similar to that of the raw materials.
Thickness test of expanded carbon layer
The experimental equipment adopts JL-JCF-3 (Bright Leide Nanjing) type building material smoke density tester to carry out open fire test on 100mm x 50mm x 10mm wood boards under the pressure of natural gas of 0.2MPa, and the test results are shown in Table 1:
TABLE 1 expanded carbon layer thickness
The main reason is that the phytic acid content in the system is reduced to generate a large amount of ammonium phytate, and when the phytic acid catalyzes a carbon source to form carbon, the urea and the ammonium phytate are decomposed to generate a large amount of gas, so that the thickness of the carbon layer is increased. When the proportion of urea is more than 12, the thickness of the carbon layer is gradually reduced, and the main reason is that a large amount of urea exists in the system, and a large amount of gas is released to burst the carbon layer when the system is heated, so that the thickness of the carbon layer is reduced.
Limiting oxygen index test
According to GB/T2406-1993, a JL-JF-5 (Bright south Beijing) type full-automatic oxygen index tester is adopted to test a sample according to GB/T2406-93 standard, and the size of the sample is 130mm multiplied by 6.5mm multiplied by 3mm. The test was repeated 5 times for each sample, and the test results are shown in table 2:
TABLE 2 oxygen index distribution
As can be seen from Table 2, the rest oxygen index of the poplar samples subjected to flame retardant treatment except for 1-3 groups reaches more than 60%, which is enough to show that the intumescent flame retardant has good flame retardant effect.
Smoke Density Performance test
The experimental equipment adopts JL-JCF-3 (Bright Leide Nanjing) type building material smoke density tester to test the smoke density under the natural gas pressure of 0.2 MPa. Each group of samples was tested 5 times and averaged.
The smoke density grade distribution is shown in figure 2, and it can be seen from the figure that the smoke density grade of the starch treatment group is far greater than that of the poplar sample, and the smoke density grades of the rest groups except 1-3 groups are greater than that of the poplar sample but smaller than that of the starch treatment group, because the expansion height of the carbon layers of 1-3 groups is not high and the cracking condition is less, and the carbon layers of the rest treatment groups are more compact and expand but generate cracks in heating, so that a large amount of smoke is released by burning wood in the shade.
The symbol means: 1-3 represents that the molar ratio of the phytic acid and the urea serving as reaction raw materials is 1, 3,1-6, 1-9, 1-12, 1-15, 1-18 and 1-20, and is similar to that of the raw materials in the prior art.
Combustion quality test
The experimental equipment adopts JL-JCF-3 (Bright Leide Nanjing) type building material smoke density tester to burn for 3min under the natural gas pressure of 0.2MPa, and the results are shown in Table 3:
TABLE 3 Mass Change before and after Combustion
As can be seen from the table, the poplar-like and starch-treated groups lost a lot of mass before and after burning, and were completely burnt. Through the flame-retardant coating layer group, the loss of less mass is enough to indicate that the flame-retardant effect is excellent, and the loss of mass is in the trend of increasing firstly and then decreasing along with the increase of the urea content, and is the same as the thickness of the carbon layer.
The preferred embodiments of the present invention disclosed above are intended to facilitate the explanation of the present invention only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. The flame retardant with the controllable thickness of the expanded carbon layer is characterized in that the preparation process of the flame retardant comprises the following steps:
1) Putting phytic acid and urea into a reaction vessel according to a certain molar ratio, heating at 90-130 ℃, condensing and refluxing for 4-8 h to obtain oily liquid;
2) Putting the obtained oily liquid into an ultralow temperature device, and freezing for 12-48 h at the temperature of-80 ℃; then drying for 12-48 h at-50 ℃ by using a freeze dryer to obtain a solid intermediate;
3) Adding the obtained solid intermediate, starch and glacial acetic acid into a proper amount of pure water according to a certain mass ratio, and heating and stirring at 85-95 ℃ for 5-20 min to obtain the required flame retardant.
2. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: the molar ratio of the phytic acid to the urea is 1 x, wherein x = 3-20;
when x =6, the solid intermediate obtained in step 2) is an ammonium phytate solid;
when x is less than 6, the solid intermediate obtained in the step 2) is phytic acid/ammonium phytate composite solid;
when x is larger than 6, the solid intermediate obtained in the step 2) is urea/ammonium phytate composite solid.
3. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 1), heating, condensing and refluxing for 6h at the temperature of 120 ℃.
4. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 2), the obtained oily liquid is put into an ultralow temperature device and is frozen for 24 hours at the temperature of minus 80 ℃.
5. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 2), a freeze dryer is used for drying for 24 hours at the temperature of minus 50 ℃.
6. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 3), the mixture is heated and stirred for 5-20 min at the temperature of 85-95 ℃.
7. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 3), the starch is at least one of potato starch, corn starch, cassava starch and wheat starch.
8. The intumescent carbon layer thickness controllable flame retardant of claim 1, wherein: in the step 3), the mass ratio of the solid intermediate, the starch and the glacial acetic acid is 5-15.
9. The intumescent carbon layer thickness controllable flame retardant of claim 8, wherein: the mass ratio of the solid intermediate to the starch to the glacial acetic acid is 10.
10. The method for preparing flame-retardant wood using the expanded carbon layer thickness-controllable flame retardant of any one of claims 1 to 9, comprising the steps of:
s1, firstly, the flame retardant is mixed according to the proportion of 0.20-0.30 g/cm 2 Smearing on the raw material wood board;
s2, drying the raw material wood board coated with the flame retardant in the shade for 2-4 hours, and then drying at 40 ℃ to obtain a dried wood board;
s3, placing the obtained dried wood board in a constant temperature and humidity box, and carrying out water balance under the conditions of temperature of 22 ℃ and humidity of 65%, wherein the balance time is more than or equal to 80h.
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